反应详情

温度

0 °C

A dry round bottom flask is charged with LiAlH4 (4 eq), and dry THF is added. The suspension is cooled down to 0° C. and a solution of compound 10 in THF is added dropwise. The reaction mixture is stirred 4 h at room temperature then cooled down to 0° C. and quenched with water, followed by 10% NaOH and then water again. The mixture is stirred overnight and the solid is filtered off. The aqueous phase is extracted with CH2Cl2, the organic extracts are collected and dried (Na2SO4). After evaporation of the solvent under reduced pressure and purification by reverse phase preparatory HPLC [6-(3-methoxyphenyl)-2-(2-morpholin-4-ylethyl)pyrimidin-4-yl]-3-pyridylamine 11 is obtained.

1. additionis added
2. temperaturethen cooled down to 0° C.
3. customquenched with water
4. stirringThe mixture is stirred overnight
5. filtrationthe solid is filtered off
6. extractionThe aqueous phase is extracted with CH2Cl2
7. customthe organic extracts are collected
8. dry with materialdried (Na2SO4)
9. customAfter evaporation of the solvent
10. customunder reduced pressure and purification by reverse phase preparatory HPLC [6-(3-methoxyphenyl)-2-(2-morpholin-4-ylethyl)pyrimidin-4-yl]-3-pyridylamine 11
11. customis obtained